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采用高分辨率连续光源石墨炉原子吸收光谱法和直接固体样品分析,对生物质样品及其灰分中的 Cd 和 Cr 进行连续测定。

Sequential determination of Cd and Cr in biomass samples and their ashes using high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample analysis.

机构信息

Instituto de Química, Universidade Federal do Rio Grande do Sul, Av. Bento Gonçalves 9500, 91501-970 Porto Alegre-RS, Brazil.

出版信息

Talanta. 2013 Oct 15;115:55-60. doi: 10.1016/j.talanta.2013.04.036. Epub 2013 Apr 19.

Abstract

High-resolution continuum source graphite furnace atomic absorption spectrometry, because of the use of only one radiation source for all elements, offers the possibility of sequential determination of two or more elements from the same sample aliquot if their volatilities are significantly different. Cd and Cr were determined sequentially in samples of biomass and biomass ashes employing direct solid sample analysis. The use of a chemical modifier was found to be not necessary, and calibration could be carried out using aqueous standard solutions. A pyrolysis temperature of 400°C and an atomization temperature of 1500°C were used for the determination of Cd; no losses of Cr were observed at this temperature. After the atomization of Cd the wavelength was changed and Cr atomized at 2600°C. The limits of detection (LOD) and quantification (LOQ) were 1.1 μg kg(-1) and 3.7 μg kg(-1), respectively, for Cd and 21 μg kg(-1) and 70 μg kg(-1), respectively, for Cr using the most sensitive line at 357.869 nm, or 90 μg kg(-1) and 300 μg kg(-1), respectively, using the less sensitive line at 428.972 nm. The precision, expressed as relative standard deviation was around 10%, which is typical for direct solid sample analysis. The values found for Cd in biomass samples were between <1.1 µg kg(-1) and 789 µg kg(-1), whereas those for Cr were between 7.9 mg kg(-1) and 89 mg kg(-1); the values found in the ashes were significantly lower for Cd, between <1.1 µg kg(-1) and 6.3 µg kg(-1), whereas the trend was not so clear for Cr, where the values were between 3.4 mg kg(-1) and 28 mg kg(-1).

摘要

高分辨率连续光源石墨炉原子吸收光谱法,由于仅使用一个辐射源即可测定所有元素,如果元素的挥发性有明显差异,则可从同一样品中顺序测定两种或更多种元素。采用直接固体样品分析,对生物质和生物质灰分样品中的 Cd 和 Cr 进行了顺序测定。研究发现,无需使用化学改性剂,即可使用水溶液标准溶液进行校准。在 400°C 的热解温度和 1500°C 的原子化温度下对 Cd 进行测定,在该温度下未观察到 Cr 的损失。在原子化 Cd 之后,改变波长并在 2600°C 下原子化 Cr。使用最灵敏的 357.869nm 波长线时,Cd 的检出限(LOD)和定量限(LOQ)分别为 1.1μgkg(-1)和 3.7μgkg(-1),Cr 的检出限(LOD)和定量限(LOQ)分别为 21μgkg(-1)和 70μgkg(-1),使用次灵敏的 428.972nm 波长线时,Cd 的检出限(LOD)和定量限(LOQ)分别为 90μgkg(-1)和 300μgkg(-1)。用相对标准偏差表示的精度约为 10%,这是直接固体样品分析的典型值。在生物质样品中 Cd 的含量在<1.1μgkg(-1)至 789μgkg(-1)之间,而 Cr 的含量在 7.9mgkg(-1)至 89mgkg(-1)之间;在灰分中 Cd 的含量明显较低,在<1.1μgkg(-1)至 6.3μgkg(-1)之间,而 Cr 的含量趋势不明显,在 3.4mgkg(-1)至 28mgkg(-1)之间。

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